CN104844404A - Method for separating hendecane, dodecane and normal decyl alcohol by continuous side rectification coupling extractive rectification - Google Patents
Method for separating hendecane, dodecane and normal decyl alcohol by continuous side rectification coupling extractive rectification Download PDFInfo
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Abstract
A method for separating hendecane, dodecane and normal decyl alcohol by continuous side rectification coupling extractive rectification comprises the following steps: (1) adding a raw material to a continuous side rectifying tower, and performing rectification pretreatment to obtain an overhead fraction 2 with a boiling range of 102.1 to 103.4 DEG C, a side fraction 3 with a boiling range of 146.7 to 147.9 DEG C, and a bottom tower fraction 4 with a boiling range of 186.2 to 187.5 DEG C at the same time, wherein content of dodecane in the side fraction 3 is more than 94.8%; (2) putting the side fraction 3 into an extractive rectifying tower, so as to obtain an overhead fraction 5 with a boiling range of 121.0 to 122.1 DEG C in the top of the tower by using glycerol as an extraction agent, wherein content of dodecane in the overhead fraction 5 is more than 99.2%, and a bottom tower fraction 6 manly contains the extraction agent; and (3) processing the bottom tower fraction 6 by using a solvent recovery tower, wherein the extraction agent is recycled in a tower reactor. According to the invention, a separation technology of continuous side rectification coupling extractive rectification is used, so that a process is simple, and separation efficiency is high. Further, content and yield of dodecane are improved, and potential for industrial production is great.
Description
Technical field
The present invention relates to a kind of chemical separating method, particularly relate to the method for a kind of continuous lateral line rectifying coupling separation of extractive distillation undecane, dodecane and positive ten alcohol.
Background technology
A large amount of front-end volatiles and mink cell focus is produced in soybean oil is produced, wherein front-end volatiles account for about 12% of total amount, containing the undecane of about 23%, about 56% dodecane and about 21% positive ten alcohol in front-end volatiles, the monomers such as dodecane are important chemical industry and pharmaceutical raw material, for the production of SL-AH, straight chain alcohol and haloalkane, as daily chemical products main raw material etc.In the past soybean oil produce in using front-end volatiles as industrial solvent or oil fuel process, not only waste important starting material, simultaneously to environment produce certain influence.
Dodecane is mainly derived from the last running (boiling point >=200 DEG C) after extraction No. 200 solvent oils, through isomerization and the preparation of rectifying combining method, because the method difficulty is large, cost is high, domestic at present only have small-scale production, output is only about 35 tons/year, and the content of product reaches 98%.Dodecane not yet forms scale production at home, basic dependence on import.
In view of the behaviour in service of front-end volatiles in current domestic soybean oil production, the invention provides the method for undecane, dodecane and positive ten alcohol in a kind of continuous lateral line rectifying coupling separation of extractive distillation soybean oil front-end volatiles.
Summary of the invention
The object of the present invention is to provide the method for a kind of continuous lateral line rectifying coupling separation of extractive distillation undecane, dodecane and positive ten alcohol, first adopt the method pre-treatment undecane of continuous lateral line rectifying, dodecane and positive ten alcohol mixtures, just divide three cuts obtaining different boiling ranges; Then adopt extraction rectifying method process mainly to comprise the cut of dodecane, be separated dodecane and positive ten alcohol, obtain more than 99.2% dodecane, this process choosing glycerine is extraction agent, and separating effect significantly improves; And adopting solvent recovery tower to reclaim glycerine, solvent cycle uses.This technique is simple, separation efficiency is high, production cost is low, having a high potential of suitability for industrialized production.
For achieving the above object, the present invention adopts following technical scheme:
A method for continuous lateral line rectifying coupling separation of extractive distillation undecane, dodecane and positive ten alcohol, step is as follows:
(1) raw material undecane, dodecane and positive ten alcohol mixed solutions add continuous lateral line rectifying tower, heat at the bottom of tower, control at the bottom of tower top, tower and side stream temperature, through rectifying pre-treatment, obtain simultaneously boiling range be the overhead fraction of 102.1 DEG C ~ 103.4 DEG C 2., boiling range be 3. the side stream of 146.7 DEG C ~ 147.9 DEG C with boiling range the be tower bottom distillate of 186.2 DEG C ~ 187.5 DEG C 4.; Wherein, side stream 3. in the content of dodecane be more than 94.8wt%;
(2) 3. side stream enters extractive distillation column, and employing glycerine is extraction agent, control tower top, column bottom temperature, extracting rectifying column overhead obtain boiling range be the overhead fraction of 121.0 DEG C ~ 122.1 DEG C 5., dodecane content is more than 99.2wt%; Obtain at the bottom of tower boiling range be the tower bottom distillate of 199.1 DEG C ~ 201.7 DEG C 6., main containing extraction agent and a small amount of dodecane, positive ten alcohol;
(3) extractive distillation column tower bottom distillate is 6. through solvent recovery tower rectification process, and 7., 8. tower reactor extraction extraction agent, then flows into extractive distillation column and recycle for solvent recovery tower overhead extraction dodecane and positive ten alcohol cuts.
In above scheme, the extraction agent in described (2) step is glycerine, and the mass ratio of extraction agent and extractive distillation column feedstock amount is 1:0.8-1.2.
By weight percentage, it consists of undecane 22 ~ 25%, dodecane 55 ~ 58% and positive ten alcohol 20 ~ 22% for described raw material undecane, dodecane and positive ten alcohol mixed solutions.
In described method, in (2) step, the pressure-controlling of extractive distillation column is 0.05 ~ 1.0atm.
In described method, in (3) step, solvent recuperation column overhead temperatures is 127.5 ~ 128.6 DEG C, and bottom temperature is 211.4 ~ 213.3 DEG C, and reflux ratio is 2 ~ 3.
First aforesaid method adopts the method pre-treatment undecane of continuous lateral line rectifying, dodecane and positive ten alcohol mixtures, and control different boiling ranges and obtain undecane, dodecane and positive ten alcohol cuts, traditional technology needs two rectifying tower just can complete this task; Two is that adopt extraction rectifying method to be separated dodecane and positive ten alcohol, this process choosing glycerine is extraction agent, and separating effect significantly improves, and can obtain more than 99.2% dodecane to just dividing the cut mainly comprising dodecane, contain positive ten alcohol on a small quantity obtained.Finally, adopt solvent recovery tower to reclaim glycerine, solvent cycle uses.Described method technique is simple, separation efficiency is high.
More specifically and more optimally say, front-end volatiles in producing for soybean oil, in its composition, undecane, dodecane and positive ten alcohol are about undecane 22 ~ 23%, dodecane 56 ~ 57% and positive ten alcohol 20 ~ 21%, adopt continuous lateral line rectifying coupling extracting rectifying to be separated, concrete operation step of the present invention is:
(1) raw material undecane, dodecane and positive ten alcohol mixed solutions add continuous lateral line rectifying tower, and control inlet amount is 10Kg/h, load D at the bottom of tower top, side line and tower
2, D
3and D
4be respectively 2.5Kg/h, 4.5Kg/h and 3.0Kg/h, tower top temperature is at 102.1 DEG C ~ 103.4 DEG C, bottom temperature is at 186.2 DEG C ~ 187.5 DEG C, side stream temperature is at 146.7 DEG C ~ 147.9 DEG C, reflux ratio 4 ~ 5, theoretical plate number is 50, feedstock position is at the 25th piece of column plate place, lateral line discharging position is at the 30th piece of column plate place, through the pre-treatment of continuous lateral line rectifying tower, can obtain boiling range is that 2. the tower top that heats up in a steamer of 102.1 DEG C ~ 103.4 DEG C divides simultaneously, boiling range be 3. the side stream of 146.7 DEG C ~ 147.9 DEG C with boiling range the be tower bottom distillate of 186.2 DEG C ~ 187.5 DEG C 4., the content of overhead fraction 2. undecane cut is>=91.40%, side stream 3. in the content of dodecane be>=94.8%, tower bottom distillate is 4. mainly containing dodecane and positive ten alcohol.
(2) 3. the side stream of continuous lateral line rectifying tower enters extractive distillation column, and feedstock amount is 4.0Kg/h, load D at the bottom of tower top and tower
5and D
6be respectively 3.8Kg/h and 4.2Kg/h, control tower top temperature at 121.0 ~ 122.1 DEG C, bottom temperature is at 199.1 ~ 201.7 DEG C, reflux ratio is 2 ~ 3, theoretical plate number is 30, and 3. side stream enters extractive distillation column position at the 15th block of plate, and extractant feed position is at the 3rd block of plate, 5. extractive distillation column overhead fraction obtains content>=99.20% of dodecane, tower reactor be tower bottom distillate containing a large amount of extraction agent, a small amount of dodecane and positive ten alcohol 6..
Described extraction solvent is glycerine, and the optimum quality ratio of extraction agent and extractive distillation column feedstock amount is 1: 1.
(3) above-mentioned extractive distillation column tower bottom distillate is 6. through solvent recovery tower process, and control inlet amount is 4.2Kg/h, load D at the bottom of tower top and tower
7and D
8be respectively 0.19Kg/h, 4.01Kg/h, tower top temperature is at 127.5 ~ 128.6 DEG C, bottom temperature is at 211.4 ~ 213.3 DEG C, feed entrance point is at the 12nd block of plate, reflux ratio 2 ~ 3, solvent recuperation column overhead be dodecane and positive ten alcohol cuts 7., tower reactor be extraction agent 8., content more than 99.70%, then flow into extractive distillation column and recycle.
Above-mentioned separation process conditions and result are as shown in Table 1 and Table 2.
The processing condition of table 1 sepn process
The composition of each cut of table 2 sepn process and content
The method of continuous lateral line rectifying coupling separation of extractive distillation undecane of the present invention, dodecane and positive ten alcohol, continuous lateral line rectifying is adopted to carry out pre-treatment, mixed alkanes is after pre-treatment, and the content being rich in dodecane cut brings up to more than 94.80%, and yield is more than 75%; Adopt extraction rectifying method to be separated dodecane and positive ten alcohol again, in extracting rectifying, adopt glycerine as extraction agent, improve separation efficiency, the content of dodecane component brings up to more than 99.2%, and yield is more than 94.5%.The inventive method technique is simple, separation efficiency is high, significantly reduces production cost, having a high potential of suitability for industrialized production.
Describe the present invention below in conjunction with specific embodiment.Protection scope of the present invention is not limited with embodiment, but is limited by claim.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of continuous lateral line rectifying and extracting rectifying integrated purification undecane, dodecane and positive ten alcohol;
In figure, 1, continuous lateral line rectifying tower, 2, extractive distillation column, 3, solvent recovery tower.
Embodiment
Below by specific embodiment, technical solutions according to the invention are further described in detail, but are necessary to point out that following examples are only for the description to summary of the invention, do not form limiting the scope of the invention.
Embodiment 1, the mixture of continuous lateral line rectifying coupling separation of extractive distillation undecane, dodecane and positive ten alcohol, each tower internal diameter is 57cm, adopt the Stainless Steel Helices of φ 3 × 3 θ type, through measuring by standards system, this height equivalent to one theoretical plate HETP=27mm, tower reactor adopts voltate regulator to control electrically heated, is undertaken quantitatively and qualitative analysis by gas chromatography-mass spectrometry chromatogram instrument.Said method comprising the steps of:
(1) 1. raw material undecane, dodecane and positive ten alcohol mixed solutions add continuous lateral line rectifying tower 1, tower reactor controls electrically heated by voltate regulator, feedstock amount and operating parameters and the results are shown in Table shown in 3,2. overhead fraction is 91.40% for undecane content, side stream 3. in the content of dodecane be 94.8%, tower bottom distillate is 4. containing dodecane and positive ten alcohol;
(2) 3. the side stream of continuous lateral line rectifying tower 1 enters extractive distillation column 2, feedstock amount and operating parameters and the results are shown in Table shown in 4, the content that 5. extractive distillation column 2 overhead fraction obtains dodecane cut is 99.60%, tower reactor be cut containing a large amount of extraction agent, dodecane and positive ten alcohol 6.;
(3) 6. the above-mentioned cut containing a large amount of extraction solvent, dodecane and positive ten alcohol processes through solvent recovery tower 3, and control inlet amount is 4.2Kg/h, load D
7and D
8be respectively 0.19Kg/h, 4.01Kg/h, tower top temperature is at 128.1 DEG C, bottom temperature is at 212.3 DEG C, feed entrance point is at the 12nd block of plate, reflux ratio is 2 ~ 3, solvent recovery tower 3 tower top be dodecane and positive ten alcohol cuts 7., tower reactor cut 8. for containing 99.7% extraction agent, then flows into extractive distillation column 2 and recycles.
Table 3 side line rectifying tower operational condition and separating resulting
Table 4 extractive distillation column operational condition and separating resulting
Embodiment 2, substantially the same manner as Example 1, but in described (2) step, the pressure-controlling of extractive distillation column 2 is 0.05atm, and extracting rectifying experimental result is shown in Table 5.
Table 5 extractive distillation column operational condition and separating resulting
Embodiment 3, substantially the same manner as Example 1, but in described (2) step, the pressure-controlling of extractive distillation column is 1.0atm, and extracting rectifying experimental result is shown in Table 6.
Table 6 extractive distillation column operational condition and separating resulting
Claims (7)
1. a method for continuous lateral line rectifying coupling separation of extractive distillation undecane, dodecane and positive ten alcohol, step is as follows:
(1) raw material undecane, dodecane and positive ten alcohol mixed solutions add continuous lateral line rectifying tower, heat at the bottom of tower, control at the bottom of tower top, tower and side stream temperature, through rectifying pre-treatment, obtain simultaneously boiling range be the overhead fraction of 102.1 DEG C ~ 103.4 DEG C 2., boiling range be 3. the side stream of 146.7 DEG C ~ 147.9 DEG C with boiling range the be tower bottom distillate of 186.2 DEG C ~ 187.5 DEG C 4.; Wherein, side stream 3. in the content of dodecane be more than 94.8wt%;
(2) 3. side stream enters extractive distillation column, employing glycerine is extraction agent, control tower top, column bottom temperature, extracting rectifying column overhead obtain boiling range be the overhead fraction of 121.0 DEG C ~ 122.1 DEG C 5., wherein the content of dodecane is more than 99.2wt%, obtain at the bottom of tower boiling range be the tower bottom distillate of 199.1 DEG C ~ 201.7 DEG C 6., main containing extraction agent and a small amount of dodecane, positive ten alcohol;
(3) extractive distillation column tower bottom distillate is 6. through solvent recovery tower rectification process, and 7., 8. tower reactor extraction extraction agent, then flows into extractive distillation column and recycle for solvent recovery tower overhead extraction dodecane and positive ten alcohol cuts.
2. the method for continuous lateral line rectifying coupling separation of extractive distillation undecane according to claim 1, dodecane and positive ten alcohol, it is characterized in that: in described (2) step, the mass ratio of extraction agent glycerine and extractive distillation column feedstock amount is 1: 0.8 ~ 1.2.
3. the method for continuous lateral line rectifying coupling separation of extractive distillation undecane according to claim 1 and 2, dodecane and positive ten alcohol, it is characterized in that, described raw material undecane, dodecane and positive ten alcohol mixed solutions are by weight percentage, it consists of, undecane 22 ~ 25%, dodecane 55 ~ 58% and positive ten alcohol 20 ~ 22%.
4. the method for continuous lateral line rectifying coupling separation of extractive distillation undecane according to claim 3, dodecane and positive ten alcohol, it is characterized in that, described raw material undecane, dodecane and positive ten alcohol mixed solutions are by weight percentage, it consists of, undecane 22 ~ 23%, dodecane 56 ~ 57% and positive ten alcohol 20 ~ 21%.
5. the method for continuous lateral line rectifying coupling separation of extractive distillation undecane according to claim 4, dodecane and positive ten alcohol, it is characterized in that, in described method, (1) step controls reflux ratio 4 ~ 5, side line theoretical number of plates of rectifying tower is 50, feedstock position is at the 25th piece of column plate place, and lateral line discharging position is at the 30th piece of column plate place; (2) step controls reflux ratio 2 ~ 3, and extractive distillation column theoretical plate number is 30, and 3. side stream enters extractive distillation column position at the 15th block of plate, and extractant feed position is at the 3rd block of plate.
6. the method for continuous lateral line rectifying coupling separation of extractive distillation undecane according to claim 1 and 2, dodecane and positive ten alcohol, it is characterized in that, in described method, in (2) step, the pressure-controlling of extractive distillation column is 0.05 ~ 1.0atm.
7. the method for continuous lateral line rectifying coupling separation of extractive distillation undecane according to claim 1 and 2, dodecane and positive ten alcohol, it is characterized in that, in described method, in (3) step, solvent recuperation column overhead temperatures is 127.5 ~ 128.6 DEG C, bottom temperature is 211.4 ~ 213.3 DEG C, and reflux ratio is 2 ~ 3.
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| CN105777472A (en) * | 2016-04-15 | 2016-07-20 | 河北工业大学 | Method for separating pentane, hexane, heptane and octane mixture system |
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